CN115625770B - Preparation method of high-strength bamboo recombined material with flame-retardant and waterproof functions - Google Patents
Preparation method of high-strength bamboo recombined material with flame-retardant and waterproof functions Download PDFInfo
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- B27N3/08—Moulding or pressing
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- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
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- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
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- B27K3/16—Inorganic impregnating agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/36—Aliphatic compounds
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- B27K3/34—Organic impregnating agents
- B27K3/38—Aromatic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/50—Mixtures of different organic impregnating agents
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- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
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- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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- B27M1/08—Working of wood not provided for in subclasses B27B - B27L, e.g. by stretching by multi-step processes
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- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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Abstract
The invention provides a preparation method of a high-strength bamboo recombined material with flame-retardant and waterproof functions, which comprises the following steps: removing bamboo green and bamboo yellow from bamboo, processing the bamboo into bamboo chips, drying the bamboo chips, putting the bamboo chips into a choline chloride-lactic acid eutectic solvent, reacting for 30-45 min at 110 ℃, and then cleaning the bamboo chips to remove part of lignin; putting the bamboo chips into an acetic acid/hydrogen peroxide mixed solution, reacting for 45 min-1 h at 80 ℃, cleaning to be neutral, and completely removing lignin; soaking the delignified bamboo chips in calcium chloride solution and sodium carbonate solution respectively, washing with water for desalting, and drying in air; after the air-dried bamboo chips are soaked in phenolic resin, the bamboo chips are dried at low temperature until the water content is 12-14%; and (3) putting the bamboo chips dried at the low temperature into a mould along the grain direction, firstly carrying out cold pressing and hot pressing, and then carrying out pressure reduction by stages, cooling and demoulding. The method shortens the delignification treatment time, and forms a hydrophobic surface on the surface of the micro-nano cellulose to obtain the high-strength bamboo recombined material with flame retardant and waterproof functions.
Description
Technical Field
The invention relates to a preparation method of a high-strength bamboo recombined material with flame-retardant and waterproof functions, belonging to the field of bamboo processing.
Background
Bamboo wood, as a sustainable biomass raw material, is gradually applied to the preparation of high-strength light structural engineering materials due to the advantages of short growth cycle, high mechanical strength, degradability and the like. However, the bamboo material as a biomass material has the defects of flammability, poor thermal stability and the like, and the application of the bamboo material in the aspects of transportation, transportation and the like is limited. At present, in order to fully utilize the advantage of excellent mechanical strength of bamboo unit components, relevant researchers impregnate phenolic resin or epoxy resin and the like into the natural bamboo after delignification treatment is carried out on the natural bamboo by utilizing hydrogen peroxide and acetic acid, so that the natural bamboo is filled into a pore structure of the bamboo to prepare a high-performance structural material. After delignification treatment, the bamboo cell tissue is separated, the specific surface area is improved, but the dimensional stability of the bamboo is poor due to a large amount of hydrophilic groups such as hydroxyl groups and the like on cellulose molecular chains in the bamboo, so that the bamboo is impregnated with resin to be filled into a bamboo void structure so as to improve the dimensional stability of the bamboo. And the traditional method for removing lignin by hydrogen peroxide and acetic acid has the problems of high concentration of pretreatment liquid, large consumption, difficult recovery and the like, and seriously pollutes the environment. Besides, related researchers fill the bamboo wood with inorganic salt ions by using a method of impregnating the bamboo wood with the inorganic salt ions in order to improve the flame retardant property of the bamboo wood, and hydroxyl groups and a porous structure in the bamboo wood provide good deposition conditions for the bamboo wood, but the dimensional stability of the bamboo wood is not obviously improved finally, and the application range of the bamboo wood is still limited. Therefore, it is very important to prepare a high-strength bamboo recombined material with flame retardant and waterproof functions.
Disclosure of Invention
The invention provides a preparation method of a high-strength bamboo recombined material with flame retardant and waterproof functions, which comprises the steps of firstly carrying out hydrogen peroxide/acetic acid treatment on bamboo wood after carrying out eutectic solvent pretreatment on the bamboo wood, greatly shortening the traditional delignification treatment time, reducing the consumption, separating the bamboo wood into bamboo chips with micro/nano cellulose network structures, then depositing calcium carbonate nanoparticles on the surfaces of micro/nano cellulose in situ by using sodium carbonate and calcium chloride, filling the inner pores of the bamboo chips and forming uniform hydrophobic layers on the surfaces, carrying out directional recombination after phenolic resin impregnation, filling the gaps between bamboo fibers and fibers, and finally carrying out hot pressing and densification to obtain the high-strength bamboo recombined material with flame retardant and waterproof functions.
The technical scheme of the invention is as follows: a preparation method of a high-strength bamboo recombined material with flame-retardant and waterproof functions comprises the following specific steps:
firstly, the green bamboo and the yellow bamboo are removed from the bamboo, then the bamboo is processed into bamboo chips with certain width, and the bamboo chips are dried until the water content is 8 to 10 percent;
secondly, placing the dried bamboo chips into a prepared choline chloride-lactic acid eutectic solvent, heating the bamboo chips to 110 ℃ through an oil bath pot device, reacting for 30-45 min, cleaning redundant reaction solution with a mixed solution of acetone and deionized water after the reaction is finished, and finally cleaning with deionized water to remove part of lignin in the bamboo chips;
thirdly, placing the bamboo chips treated by the eutectic solvent into an acetic acid/hydrogen peroxide mixed solution, heating the bamboo chips to 80 ℃ through a water bath device, reacting for 45 min-1 h, and cleaning the bamboo chips to be neutral by using deionized water after the reaction is finished, so as to completely remove lignin in the bamboo chips;
and (IV) respectively putting the delignified bamboo chips into calcium chloride solution for vacuum impregnation for 45-60 min, then impregnating at normal pressure for 45-60 min, and putting the impregnated bamboo chips into a drying oven for drying. Then, putting the mixture into a sodium carbonate solution for vacuum impregnation for 45-60 min, then impregnating the mixture for 45-60 min at normal pressure, washing the mixture for desalination after the reaction is finished, and drying the mixture in air after the desalination;
fifthly, putting the air-dried calcium carbonate mineralized bamboo chips into phenolic resin, immersing the sample in the phenolic resin completely for 10-15 min under normal pressure, vacuum immersing for 6-10 min, and drying the bamboo chips at low temperature until the water content is 12% -14% after immersion;
and (VI) putting the bamboo chips dried at the low temperature into a mould along the grain direction, putting the bamboo chips into a flat vulcanizing machine, cold-pressing the bamboo chips for 15 to 20 minutes at 0.5MPa, forming the bamboo chips, then hot-pressing the bamboo chips for 5 to 10 minutes at the high temperature of between 130 and 140 ℃ under the unit pressure of 4.0MPa, and finally reducing the pressure by stages, cooling the bamboo chips to between 40 and 50 ℃ and demoulding the bamboo chips to prepare the high-strength bamboo recombined material with the flame-retardant and waterproof functions.
The invention has the advantages that:
the bamboo chips are treated by using a eutectic solvent and combining a traditional delignification method, so that lignin and partial hemicellulose in the bamboo are removed, the specific surface area of the bamboo is improved, the bamboo is separated into the bamboo chips with the micro/nano cellulose network structure, and a good condition is provided for the deposition of calcium carbonate. In addition, the pretreatment of the eutectic solvent greatly shortens the time of traditional delignification, reduces the consumption and solves the problem of environmental pollution to a certain extent.
Secondly, the bamboo chips are mineralized in situ by using calcium chloride and sodium carbonate, so that calcium carbonate nanoparticles are deposited on the surfaces of the micro/nano cellulose in the bamboo chips, and the flame retardant property of the bamboo materials can be obviously improved; and then further impregnating phenolic resin, performing hot-pressing recombination, filling gaps between the bamboo fibers, improving the dimensional stability and the mechanical property of the bamboo, and finally forming the high-strength bamboo recombined material with flame retardant and waterproof functions.
And (III) the surface of the micro-nano cellulose in the bamboo chip is uniformly covered with nano calcium carbonate particles through process control to form a hydrophobic layer, so that the hydrophobic property of the bamboo chip is enhanced to a certain extent, and the dimensional stability of the bamboo chip is improved.
Detailed Description
A preparation method of a high-strength bamboo recombined material with flame-retardant and waterproof functions comprises the following steps:
firstly, the green bamboo and the yellow bamboo are removed from the bamboo, then the bamboo is processed into bamboo chips with certain width, and the bamboo chips are dried until the water content is 8 to 10 percent;
putting the dried bamboo chips into a prepared choline chloride-lactic acid eutectic solvent, heating the mixture to 110 ℃ through an oil bath device, reacting for 30-45 min, cleaning redundant reaction solution with a mixed solution of acetone and deionized water after the reaction is finished, and finally cleaning with deionized water to remove part of lignin in the bamboo chips;
thirdly, placing the bamboo chips treated by the eutectic solvent into an acetic acid/hydrogen peroxide mixed solution, heating the bamboo chips to 80 ℃ through a water bath device, reacting for 45 min-1 h, and cleaning the bamboo chips to be neutral by using deionized water after the reaction is finished, so as to completely remove lignin in the bamboo chips;
and (IV) respectively putting the delignified bamboo chips into calcium chloride solutions with different concentrations for vacuum impregnation for 45-60 min, then impregnating at normal pressure for 45-60 min, and putting the impregnated bamboo chips into a drying oven for drying. Then, putting the mixture into sodium carbonate solutions with different concentrations for vacuum impregnation for 45-60 min, then carrying out normal pressure impregnation for 45-60 min, carrying out water washing desalination treatment after the reaction is finished, and carrying out air drying after the desalination treatment;
fifthly, putting the air-dried calcium carbonate mineralized bamboo chips into phenolic resin, immersing the sample in the phenolic resin completely for 10-15 min under normal pressure, vacuum immersing for 6-10 min, and drying the bamboo chips at low temperature until the water content is 12% -14% after immersion;
and (VI) putting the bamboo chips dried at the low temperature into a mould along the grain direction, putting the bamboo chips into a flat vulcanizing machine, cold-pressing the bamboo chips for 15 to 20 minutes at 0.5MPa, forming the bamboo chips, then hot-pressing the bamboo chips for 5 to 10 minutes at the high temperature of between 130 and 140 ℃ under the unit pressure of 4.0MPa, and finally reducing the pressure by stages, cooling the bamboo chips to between 40 and 50 ℃ and demoulding the bamboo chips to prepare the high-strength bamboo recombined material with the flame-retardant and waterproof functions.
Example 1
Firstly, removing bamboo green and bamboo yellow from bamboo, and processing the bamboo into bamboo chips with the width of 20 mm. Drying the bamboo chips at 100 deg.C until the water content is about 8%. Finally, the mixture is put into a climate box with the temperature of 25 ℃ and the relative humidity of 65 percent for balanced treatment.
And (II) preparing a choline chloride/lactic acid mixed solution with a molar ratio of 1.
And (III) preparing an acetic acid/hydrogen peroxide mixed solution with a volume ratio of 1.
And (IV) respectively preparing a calcium chloride solution with the concentration of 0.1mol/L and a sodium carbonate solution with the concentration of 0.1mol/L at room temperature. Then dipping the dried bamboo chips in the step (III) into a calcium chloride solution, and keeping vacuum dipping for 60min, wherein the pressure is-0.1 MPa; taking out, soaking at normal temperature and normal pressure for 60min, taking out the test piece, and drying in a drying oven. Then dipping the mixture into a sodium carbonate solution for vacuum dipping for 60min, wherein the pressure is-0.1 MPa; taking out, soaking at normal temperature and normal pressure for 60min, washing with water for desalting, and air drying. Finally, the mixture is put into a constant temperature and humidity box with the temperature of 20 +/-2 ℃ and the humidity of 60 +/-5 percent for storage and standby.
Fifthly, putting the bamboo chips dried in the step four into phenolic resin, immersing the bamboo chips in the phenolic resin completely for 10min under normal pressure, immersing the bamboo chips for 10min under vacuum, and drying the bamboo chips at a low temperature of no more than 80 ℃ until the water content is about 12 percent after immersion;
and (VI) loading the bamboo chips dried at the low temperature into a mould according to the upper layer and the lower layer of the multi-layer assembly along the grain direction, transversely splicing and longitudinally lengthening the bamboo chips in each layer, placing the bamboo chips into a flat vulcanizing machine, cold-pressing the bamboo chips for 15min under 0.5MPa, then forming, raising the temperature of the press to 140 ℃, raising the temperature rate to 20 ℃/min, raising the hot-pressing time to 10min, and reducing the pressure per unit to 4.0MPa, and finally reducing the pressure by stages, cooling the bamboo chips to about 40 ℃ and demoulding to prepare the high-strength recombined bamboo material with the flame retardant and waterproof functions.
The tensile strength and the tensile modulus of the prepared recombined bamboo are 536.8MPa and 58.6GPa respectively, the static bending strength and the elastic modulus are 358.6MPa and 34.2GPa respectively, the water absorption rate is 5.36%, the thickness expansion rate is 2.14%, the width expansion rate is 0.61%, and the heat release rate and the total heat release rate are 390.2Kw/m respectively 2 And 57.4MJ/m 2 The smoke release rate and the smoke release amount are respectively 0.017m 2 S and 2.34m 2 PerKg, the maximum average heat dissipation rate is 210.5MJ/m 2 。
Example 2
Example 2 differs from example 1 in that: under the condition of room temperature, a calcium chloride solution with the concentration of 0.5mol/L and a sodium carbonate solution with the concentration of 0.5mol/L are respectively prepared.
The tensile strength and the tensile modulus of the prepared recombined bamboo are 583.6MPa and 63.6GPa respectively, the static bending strength and the elastic modulus are 374.8MPa and 39GPa respectively, the water absorption rate is 2.19%, the thickness expansion rate is 0.68%, the width expansion rate is 0.13%, and the heat release rate and the total heat release amount are 302.6Kw/m respectively 2 And 47.9MJ/m 2 The smoke release rate and the smoke release amount are respectively 0.009m 2 S and 1.25m 2 PerKg, maximum average heat dissipation rate of 189.7MJ/m 2 。
Example 3
Example 3 differs from example 1 in that: under the condition of room temperature, a calcium chloride solution with the concentration of 0.9mol/L and a sodium carbonate solution with the concentration of 0.9mol/L are respectively prepared.
The prepared recombined bamboo has the tensile strength and the tensile modulus of 543.8MPa and 49.8GPa respectively, the static bending strength and the elastic modulus of 364.2MPa and 35.6GPa respectively, the water absorption of 5.47 percent, the thickness expansion rate of 2.24 percent, the width expansion rate of 0.72 percent, and the heat release rate and the total heat release rate of 378.4Kw/m respectively 2 And 52.3MJ/m 2 The smoke release rate and the smoke release amount were 0.015m 2 S and 1.92m 2 PerKg, the maximum average heat dissipation rate is 202.3MJ/m 2 。
Example 4
Example 4 differs from example 1 in that: under the condition of room temperature, a calcium chloride solution with the concentration of 1.3mol/L and a sodium carbonate solution with the concentration of 1.3mol/L are respectively prepared.
The tensile strength and the tensile modulus of the prepared recombined bamboo are 529.4MPa and 47.6GPa respectively, the static bending strength and the elastic modulus are 360.8MPa and 33.8GPa respectively, the water absorption rate is 6.21%, the thickness expansion rate is 2.67%, the width expansion rate is 0.87%, and the heat release rate and the total heat release rate are 342.5Kw/m respectively 2 And 49.1MJ/m 2 The smoke release rate and the smoke release amount were 0.012m, respectively 2 S and 1.64m 2 Kg, the maximum average heat dissipation rate is 195.8MJ/m 2 。
Claims (5)
1. A preparation method of a high-strength bamboo recombined material with flame-retardant and waterproof functions comprises the following steps: the method is characterized by comprising the following steps:
firstly, the green bamboo and the yellow bamboo are removed from the bamboo, then the bamboo is processed into bamboo chips with certain width, and the bamboo chips are dried until the water content is 8 to 10 percent;
putting the dried bamboo chips into a prepared choline chloride/lactic acid eutectic solvent, heating the mixture to 110 ℃ through an oil bath device, reacting for 30-45 min, cleaning redundant reaction solution with a mixed solution of acetone and deionized water after the reaction is finished, and finally cleaning with deionized water to remove part of lignin in the bamboo chips;
thirdly, placing the bamboo chips treated by the eutectic solvent into an acetic acid/hydrogen peroxide mixed solution, heating the bamboo chips to 80 ℃ through a water bath device, reacting for 45 min-1 h, and cleaning the bamboo chips to be neutral by using deionized water after the reaction is finished, so as to completely remove lignin in the bamboo chips;
putting the delignified bamboo chips into a calcium chloride solution for vacuum impregnation for 45-60 min, then impregnating at normal pressure for 45-60 min, and putting the impregnated bamboo chips into a drying box for drying; then, putting the mixture into a sodium carbonate solution for vacuum impregnation for 45-60 min, then impregnating the mixture for 45-60 min under normal pressure, washing the mixture for desalination after the reaction is finished, and drying the mixture in the air after the desalination;
fifthly, putting the air-dried calcium carbonate mineralized bamboo chips into phenolic resin, immersing the sample in the phenolic resin completely for 10-15 min under normal pressure, vacuum immersing for 6-10 min, and drying the bamboo chips at low temperature until the water content is 12% -14% after immersion;
and (VI) putting the bamboo chips dried at the low temperature into a mould along the grain direction, putting the bamboo chips into a flat vulcanizing machine, cold-pressing the bamboo chips for 15 to 20 minutes at 0.5MPa, forming the bamboo chips, then hot-pressing the bamboo chips for 5 to 10 minutes at the high temperature of between 130 and 140 ℃ under the unit pressure of 4.0MPa, and finally reducing the pressure by stages, cooling the bamboo chips to between 40 and 50 ℃ and demoulding the bamboo chips to prepare the high-strength bamboo recombined material with the flame-retardant and waterproof functions.
2. The method for preparing the high-strength bamboo recombined material with the flame-retardant and waterproof functions as claimed in claim 1, wherein the step (one) comprises the following specific contents:
removing bamboo green and bamboo yellow from bamboo, and processing into bamboo chips with width of 20 mm; drying the bamboo chips at 100 ℃ until the water content is 8-10%; and finally, placing the mixture into a climate box with the temperature of 25 ℃ and the relative humidity of 65% for balanced treatment.
3. The method for preparing the high-strength bamboo recombined material with the flame-retardant and waterproof functions as claimed in claim 1, wherein the second step comprises the following specific contents:
preparing a choline chloride/lactic acid mixed solution with a molar ratio of 1.
4. The method for preparing the high-strength bamboo recombined material with the flame-retardant and waterproof functions as claimed in claim 1, wherein the third step comprises the following specific contents:
preparing an acetic acid/hydrogen peroxide mixed solution with a volume ratio of 1.
5. The method for preparing the high-strength bamboo recombined material with the flame-retardant and waterproof functions as claimed in claim 1, wherein the fourth step comprises the following specific contents:
respectively preparing a calcium chloride solution and a sodium carbonate solution with the concentration of 0.1-1.3 mol/L at room temperature; then dipping the bamboo chips dried in the step (III) into a calcium chloride solution, and keeping vacuum dipping for 45-60 min at the pressure of-0.1 MPa; taking out the test piece, soaking the test piece for 45-60 min at normal temperature and normal pressure, taking out the test piece, and drying the test piece in a drying box; then dipping the mixture into a sodium carbonate solution for vacuum dipping for 45-60 min, wherein the pressure is-0.1 MPa; taking out, soaking at normal temperature and normal pressure for 45-60 min, washing and desalting the treated bamboo chips after the reaction is finished, and drying in air after the desalting treatment; finally, the mixture is put into a constant temperature and humidity box with the temperature of 20 +/-2 ℃ and the humidity of 60 +/-5 percent for storage and standby.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211549521.3A CN115625770B (en) | 2022-12-05 | 2022-12-05 | Preparation method of high-strength bamboo recombined material with flame-retardant and waterproof functions |
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